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1、Chapter11Assigningmolecularstructuresusingoneandtwo-dimensionalNMRdataSomeselected2DNMRexperimentsexperimentsF1F2mechanism1.HomonuclearH,H2dJ-δδHJHHnJHH(n>2)2.H,HCOSYδH,JHHδH,JHHnJHH(n=2,3)3.LongrangeCOSYδH,JHHδH,JHHnJHH(n>3)4.H,HrelayδH,JHHδH,JHHnJHH(n=2,3)5.NOESY(1DnOediff.)δH
2、,JHHδH,JHHnOe(=f.r-6)HH6.C,HCOSY(HMQC)δCδH,JHH1JCH7.Long-rangeC,HCOSYδHδHnJCH(n>1)(COLOC)(HMBC)8.HeteronuclearrelayδCδH,JHHnJCH(n=2,3);1JCH9.HOESYδCδH,JHHnOe(=f.r-6)CHF1D.Q10.2D-INADEQUATEδC,JCC1JccF2δcAssigning1HNMRSpectrumofSucroseGF1121f3(J3a,4a)4g1(J1e,2a)21111HNMRAssigning1
3、H,1HCOSY90oSpectrumofSucrosef3f3,4f4Gf5g5f6,5g6,5Ff4,5f6F1g6g5,4δHg3f5,6g5,6g2,3g1,2g2g3,4g4F2δHAssigning1H,1H2DJ-δSpectrumofSucroseFGJ3,4J4,5J4,5J5,4J5,6J5,4J2,1J3,4J4,3J3,2J4,3J5,6J2,3F1f3f4f5g5g3g2g4HzJH,HF2δHAssigning13C,1H2DJ-δSpectrumofSucroseGF1F1JC,Hf2(Hz)F2δCAssigning13
4、C,1HCOSYSpectrumofSucroseGgH4,C4gH2,C2fH1,C1FgH3,C3fH6,C6fH5,C5gH5,C5fH4,C4gH6,C6fH3,C3F1δHf5gH1,C1F2δCAssigningCOLOCSpectrumofSucroseδ13CGg4G6Ff3F1f4F6g3G5,g6G4g3g1g4G2g1G5g1g2g4G3f3f5F4f3f4f1F3f4f6F5G1g1f1F2(F2,g1)F2F2δ1HAssigningINADEQUATESpectrumofSucroseF1D.Q.GFF2G1F2δ13CAs
5、signing1Hand13CNMRSpectraofMenthol310COH20HC33H3δ1Hδ13CAssigning1H,1HCOSYSpectrumofMenthol31099,10::42α,2β4,5β1,2α31,6α5α6β1,75α,5β6β,6α2βF184,8δ1H8,108,933,2β3,43,2αF2δ1HAssigningLongrange1H,1HCOSYSpectrumofMenthol108371,74J9,103F110,89,8δ1HF2δ1HAssigningINADEQUATESpectrumofMen
6、thol712653489103F1D.Q.F2δ13CAssigning13C,1HCOSYSpectrumofMenthol7109265348134261857109C3,H3C8,H83C2,H2eF1C6,H6eC5,H5eδ1HC4,H4C1,H1C10,H10C5,H5aC2,H2aC6,H6aC7,H7C9,H9F2δ13CAssigningLong-range13C,1HCOSY(COLOC)SpectrumofMentholF1δ1H6β,5α382β4199C9,H1010C10,H975C5,H438C8,H10C8,H91C1
7、,H6βC1,H7F2δ13C6C6,H2β2C2,H6βC2,H74C4,H10C4,H9AssigningH-H-CRelaySpectrumofMenthol9382β6β5α149H8,C910H8,C10H1,C775H6,C5H4,C58H4,C8H9,C8H10,C8H2β,C1H6,C1H2α,C1136F2δ13CH3,C22H3,C4H5α,C4H5β,C44F1δ1HAssigning1H,1H2DJ-δSpectrumofMenthol10739386β5α2β14J4,8J3,2βJ4,5αJ3,4J4,3J7,1J4,5βJ
8、9,8J3,2αH7H3H4H10H9JHH(Hz)J10,8δ1HAssigningLong
